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Author Topic: P2P or L-PAC  (Read 222 times)

R.Esposito

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P2P or L-PAC
« on: September 05, 2012, 06:24:08 AM »
Hi, I work now on synthesis "(1R,2S)-(-)-ephedrine HCL".
I would like to try out reductive amination of Al / Hg, but the problem is that the amination is often associated with P2P.

P2P (1-phenylpropan-2-one) is (C9H10O) I have some L-PAC (1-hydroxy-1-phenyl-propan-2-one) is (C9H10O2).

I feel that these two oxygen molecules are able to double amination this mean very much. It can be used in Al / Hg for L-PAC?

Specifically, I am referring to J. Chem. Educ. 51, 671 (1974).
https://www.erowid.org/archive/rhodium/chemistry/amph.alhg.html

Thanks for reply.
« Last Edit: September 05, 2012, 06:32:19 AM by R.Esposito »

Assyl Fartrate

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Re: P2P or L-PAC
« Reply #1 on: September 05, 2012, 08:51:57 AM »
If you throw P2P in a fire, it makes meth. Why don't you give it a try...
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R.Esposito

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Re: P2P or L-PAC
« Reply #2 on: September 05, 2012, 09:30:59 AM »
I have only L-Phenylacetylcarbinol (L-PAC). I tried catalytic hydrogenation on Raney Nickel with methylamine 2.5 purity at 30kg/cm2 hydrogen. I'm working with hydrogen reactor.

It would be best to perform a reductive amination with catalytic hydrogenation L-PAC equal to d-meth. Or the (+)-pseudo HCl.

Unfortunately, Al / Hg molar excess of amination I found only for P2P. I have no P2P.
« Last Edit: September 05, 2012, 09:33:36 AM by R.Esposito »

Wizard X

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Re: P2P or L-PAC
« Reply #3 on: September 06, 2012, 01:21:40 AM »
Quote from: R.Esposito on September 05, 2012, 09:30:59 AM
I have only L-Phenylacetylcarbinol (L-PAC). I tried catalytic hydrogenation on Raney Nickel with methylamine 2.5 purity at 30kg/cm2 hydrogen. I'm working with hydrogen reactor.

It would be best to perform a reductive amination with catalytic hydrogenation L-PAC equal to d-meth. Or the (+)-pseudo HCl.

Unfortunately, Al / Hg molar excess of amination I found only for P2P. I have no P2P.


http://en.wikipedia.org/wiki/Phenylacetylcarbinol

1-hydroxy-1-phenyl-propan-2-one


(R)-PAC or (R)-(?)-phenylacetylcarbinol is identical to l-PAC, referring to the outdated d/l system. (R)-PAC is the levo-rotating isomer of phenylacetylcarbinol.

The IUPAC name of phenylacetylcarbinol is 1-hydroxy-1-phenylpropan-2-one. Synonyms are 1-hydroxy-1-phenyl-2-propanone and 1-Hydroxy-1-phenylacetone.

www.erowid.org/archive/rhodium/pdf/benzaldehyde.l-pac.pdf

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R.Esposito

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Re: P2P or L-PAC
« Reply #4 on: September 06, 2012, 06:09:14 AM »
It's strange to me that everything comes out as it should. I work with absolutely exact procedure and the result is negligible. I think there is a problem with reductive amination.

Goldmember

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Re: P2P or L-PAC
« Reply #5 on: September 06, 2012, 12:37:04 PM »
Quote from: Assyl Fartrate on September 05, 2012, 08:51:57 AM
If you throw P2P in a fire, it makes meth. Why don't you give it a try...

Tried it. Doesnt work as advertised. :o


Check the patent office for a step by step.
Gustav Hildebrandt and Wilfrid Klavehn are your guys. US1956950 is their number.

 Al/Hg is how it was done way back when. :-\ If this is actually what you are looking for.
« Last Edit: September 06, 2012, 12:39:27 PM by Goldmember »

java

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Re: P2P or L-PAC
« Reply #6 on: September 06, 2012, 01:46:43 PM »
Reference Information

Manufacture of L-levo-phenyl-2-methylaminepropanol-1
US Patent 1956950
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R.Esposito

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Re: P2P or L-PAC
« Reply #7 on: September 11, 2012, 05:27:05 AM »
Thanks for the response.

I'm trying to direct reductive amination of L-PAC in the reactor at Raney Nickle and Palladium.
I work according to the patent: US2509309 (attached below) ex.II .
I am unable to isolate ephedrine in free base with a melting point of about 40 ° C, always I can only (-)-ephedrine HCl with a melting point of 218 ° C by means of hydrochloric acid. Yield bothering me too :-( The reactor volume 3L most trying hydrogenate 200 g L-PAC, other substances multiply. Yield me around 30-40% in the form of HCL :-(

The (-)-ephedrine HCl can be reduced to d-meth ..... only in a closed reaction using hydriodic acid and red phosphorus. I need ephedrine, which can be reduced to d-meth ..... with iodine, red phosphorus, phosphoric acid and boiling classic way.

For example, it is nice to work with (+)-pseudoephedrine hydrochloride to d-meth.
« Last Edit: September 11, 2012, 05:28:53 AM by R.Esposito »
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